818 IC Pump Manual 8.818.
Metrohm AG CH-9101 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com 818 IC Pump 5.818.0110 Program Manual 8.818.1023 11.
Teachware Metrohm AG CH-9101 Herisau teachware@metrohm.com This documentation is protected by copyright. All rights reserved. Although all the information given in this documentation has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please send us your comments using the address given above. Documentation in additional languages can be found on http://products.metrohm.com under Literature/Technical documentation.
Table of contents Table of contents 1 Introduction .................................................... 1 1.1 1.2 1.3 Instrument description ............................................................. 1 Parts and controls .................................................................... 2 Information about the Instructions for Use ............................. 4 1.4 Safety notes .............................................................................. 6 1.3.1 1.3.2 1.4.1 1.4.2 Organization .
Table of contents 5 Interfaces ..................................................... 31 5.1 5.2 RS 232 interface...................................................................... 31 5.1.1 5.1.2 Data transmission protocol......................................................... 31 Pin assignment............................................................................ 32 5.2.1 5.2.2 Functions.....................................................................................
1.1 Instrument description 1 Introduction 1.1 Instrument description The 818 IC Pump is a serial dual piston pump especially developed for ion chromatography and optimized for use with Metrohm ion chromatographic instruments (e.g. 819 IC Detector and 820 IC Separation Center). The 818 IC Pump operates with minimal residual pulsation and has an excellent flow constancy. All wet parts of the pump are metal free. The 818 IC Pump is completely remote controlled by the Metohm software «IC Net» (version 2.
1 Introduction 1.2 Parts and controls In this section you will find the numbers and designations of the parts and controls of the 818 IC Pump. The numbering applies throughout the instructions for use, i.e. bold numbers in the text (e.g. 11) refer to the parts and controls illustrated here. 1 2 3 6 Fig. 1: 7 8 5 9 Front of 818 IC Pump 1 Mains pilot lamp Lights up when instrument is switched on 2 Purge valve 3 Connection capillary to injection valve of IC system.
1.2 Parts and controls 10 12 11 13 Fig. 2: 14 15 16 17 18 Rear of 818 IC Pump 10 Fuse cover Changing the fuses, see section 2.6.2. Mains switch For switching instrument on/off: I = ON 0 = OFF Mains connector For mains connection see section 2.6. 11 Mains voltage selector Voltage selection see section 2.6.1. 12 Serial number 13 Control interface details see section 5.2. 818 IC Pump / 8.818.
1 Introduction 1.3 Information about the Instructions for Use Please read through these Instructions for Use carefully before operating the 818 IC Pump. The Instructions for Use contain information and warnings to which the user must pay attention in order to assure safe operation of the instrument. 1.3.1 Organization These 8.818.
1.3 Information about the Instructions for Use 1.3.2 Notation and pictograms The following notations and pictograms (symbols) are used in these Instructions for Use: Range Menu item, parameter or entry value in «IC Net» program SYSTEM STATE Program window in «IC Net» program Button in «IC Net» program 10 Part or control of 818 Danger/Warning This symbol indicates a possible risk of death or injury to the user and possible damage to the instrument or its components by electricity.
1 Introduction 1.4 Safety notes 1.4.1 Electrical safety While electrical safety in the handling of the 818 IC Pump is assured in the context of the specifications IEC 1010-1 (protection class 1, degree of protection IP40), the following points should be noted: • Mains connection Set the mains voltage and check the mains fuse and mains connection in accordance with the instructions in section 2.6.
2.1 Setting up the instrument 2 Installation 2.1 Setting up the instrument 2.1.1 Packaging The 818 IC Pump is supplied together with the separately packed accessories in special packagings containing shock-absorbing foam linings designed to provide excellent protection. The actual instrument is packed in an evacuated polyethylene bag to prevent the ingress of dust. Please store all these special packagings as only they assure transport of the instruments free from damage. 2.1.
2 Installation 2.2 Mounting the pump head 1 Remove the transportation lock To ensure that the pump drive is not damaged during transport a black plastic block is mounted in place of the pump head on the right side of the 818 IC Pump front panel. This transport safeguard block has to be removed after undoing the four screws 9. To avoid any damage to the pump head, the protective block must be remounted if the pump has to be moved any great distance. 2 Mounting the pump head The Pump Head 8 (6.2824.
2.3 Attaching the accessories 2.3 Attaching the accessories 2.3.1 Capillaries Some of the connections under high pressure between the 818 IC Pump and the IC system must be set up by the user, see section 2.4. For that the 6.1831.010 PEEK capillary (i.d. = 0.25 mm, o.d. = 1/16", length = 3 m) supplied in the accessories of the 818 IC Pump can be used. Capillaries fitted with new connectors must have a perfectly flat cut surface. For PEEK capillaries it is best to use the 6.2621.
2 Installation 6.2744.010 PEEK compression fittings can be used. The flow direction is arbitrary. The pulsation dampener is positioned in the interior of the 820 IC Separation Center on the base below the injection valve (see 819/820 Instructions for Use). The pulsation dampener is filled with isopropanol when new. Rinse your IC system carefully after the first installation of a new pulsation dampener. 2.3.3 Filter unit PEEK The 6.2821.120 Filter unit PEEK 24 supplied (see Fig.
2.4 Connecting the tubing 2.4 Connecting the tubing 2.4.1 Connection to injection valve It is recommended to use 6.1831.010 PEEK capillaries, a 6.2620.150 Pulsation dampener (see section 2.3.2), and a Filter unit PEEK (see section 2.3.3) to connect the 818 IC Pump to the injection valve of the 820 IC Separation Center. Proceed as follows: 3 24 25 820 818 Fig. 5: Connection to injection valve 3 Connection capillary to 820 IC Separation Center. PEEK capillary (6.1831.010) 24 Filter unit PEEK (6.
2 Installation 2.4.2 Connection to eluent container The 6.1834.000 Aspirating tubing (i.d. = 1.5 mm, o.d. = 2.5 mm, length = 1.2 m) supplied is slid over the aspirating capillary 7. The 6.2821.090 Aspirating filter supplied is screwed onto the other end of the tubing. The end of the tubing with the aspirating filter is then introduced in the eluent container. Only degassed (with N2, He or vacuum) and microfiltered (0.
2.5 Electrical connection 2.5 Electrical connection Switch off both devices before connecting the 818 IC Pump to another instrument. 2.5.1 Connection to 830 IC Interface The 818 IC Pump is normally integrated into the modular IC system via 830 IC Interface. Connect the RS 232 interface 17 of the 818 IC Pump with a free RS 232 interface at the 830 IC Interface using the 6.2134.080 or 6.2134.090 cable according to the figure below.
2 Installation 2.5.2 Connection to PC The 818 IC Pump can also be connected directly to a PC. Connect the RS 232 interface 17 of the 818 IC Pump with a free COM port at the PC using the 6.2125.110 (for 9 pin COM port connector) or 6.2125.060 cable (for 25 pin COM port connector) according to the figure below. To ensure proper functioning of the communication between the PC and 818 IC Pump, the sliding switch 16 on the IC pump must be set to "RS 232". 818 6.2125.110/6.2125.060 CURRENT LOOP RS 232 Fig.
2.6 Mains connection 2.6 Mains connection Follow the instructions below for connecting to the power supply. If the instrument is operated with a mains voltage set wrongly and/or wrong mains fuse, there is a danger of fire! 2.6.1 Setting the mains voltage Before switching on the 818 IC Pump for the first time, check whether the mains voltage set on the instrument (can be read in the mains voltage selector 11) matches the local mains voltage.
2 Installation 2.6.2 Fuses The 818 IC Pump contains two fuses built in as standard, either of type 0.25 AT (for 230 V: 0.25 A, slow-blow, Metrohm ordering number U.600.0010) or 0.5 AT (for 110 V: 0.5 A, slow-blow, Metrohm ordering number U.600.0013). Ensure that the two fuses correspond to the fuse type specified for the local mains voltage (see also Fig. 2).
2.7 Software installation 2.7 Software installation The PC program «IC Net 2.3» is required for the operation of the 818 IC Pump. This program runs under Windows 2000 and Windows XP operating systems and is installed according to section 1.4.2 of the Instructions for Use 8.110.8283 from the Metrodata software «IC Net 2.3». The installation of 818 IC Pump is described in section 6.1.2 of the Instructions for Use 8.110.8283 from the Metrodata software «IC Net 2.3».
3 Operation 3 Operation The operation of 818 IC Pump is made completely via the Metrohm software «IC Net». This section describes only the most important points concerning the operation of the 818 IC Pump. For further details please refer to the «IC Net» Instructions for Use and to the on-line help in the PC program. 3.1 Switch instrument on/off The 818 IC Pump is switched on and off using mains switch 10 on the rear of the instrument (sse Fig. 2).
3.3 Settings in the "818 IC Pump" window Settings The Settings tab of the 818 IC Pump window contains basic settings of the 818 IC Pump. Pressure Flow Live display of current pressure in MPa. Live display of current flow in mL/min. New flow A new flow can be set by moving the scroll bar, by entering a value or by changing the value using the up and down arrows. Entry range: 0.01 ... 5.00 mL/min Min/Max pressure The minimum and maximum pressure limit for the 818 IC Pump can be set in steps of 0.1 MPa.
3 Operation switched off. At the same time, the Pressure field color in the 818 settings window is changed to the value set for Out of range. Send current parameters immediately to the 818 IC Pump (only available if pump is running). Parameters are not stored in the system file (*.smt) as long as the file is not saved. Set current parameters and start 818 IC Pump drive. Stop 818 IC Pump drive.
3.3 Settings in the "818 IC Pump" window ENABLED Enable program start (a disabled program is not started). Add new program instruction. Delete selected program instruction. Test the time program (error messages are displayed if program is wrong). List of program instructions The following program instructions can be added to the time program on the Program page: Befehl Parametereintrag Bedeutung Pump on, off Switch the high pressure pump on or off. Flow 0.01 ...
3 Operation Advanced The Advanced tab of the 818 IC Pump window is only available for a connected system. Correction factor Flow correction factor to adjust the displayed flow to the actual flow measured with the aid of a measuring cylinder. Entry range: 0.90 ... 1.10 Correction factor = Displayed flow rate (in mL/min) Measured flow rate (in mL/min) Send current Correction factor value to the 818 IC Pump. This parameter is not stored in the system file (*.smt) as long as the file is not saved.
4.1 Practical notes 4 Notes – Maintenance – Faults 4.1 Practical notes 4.1.1 Protection against foreign particles To protect the column against foreign particles which could have an adverse influence on the separation efficiency, we advise you to subject both the eluents and all samples to microfiltration (0.45 µm filter) and to siphon the eluent through the 6.2821.090 Aspirating filter.
4 Notes – Maintenance – Faults valves, pressure rise and in extreme cases to scratched pistons. It is thus essential to ensure that no precipitates can appear, e.g. when the eluent is changed. Solutions used in direct succession must therefore be miscible. If the system has to be rinsed with an organic solution, several solvents with increasing or decreasing lipophilic character may possibly have to be used (e.g. water ↔ acetone ↔ chloroform). 4.2 Maintenance and servicing 4.2.
4.2 Maintenance and servicing 4.2.2 Maintenance work at the pump head In many cases, an unstable baseline (pulsation, flow fluctuations) can be traced to contaminated valves or faulty, leaky piston seals. For cleaning contaminated valves and/or replacement of wear parts such as pistons, piston seals and valves, proceed as follows: 1 Detach pump head Unscrew connection capillary 6 from the pump head 8 with the aid of the ¼" wrench (see Fig. 1).
4 Notes – Maintenance – Faults 37 8 36 26 27 28 29 30 31 32 33 34 35 37 Fig. 8: Components of the pump head A 8 38 39 34 34 B 39 C 38 Fig. 9: 26 Replacement of the piston seal 34 818 IC Pump / 8.818.
4.2 Maintenance and servicing 8 Pump head 6.2824.100 (6.2824.030) 33 Piston guide sleeve (4.709.4370) 26 Screw for piston cartridge 30. 34 Piston seal 6.2741.020 27 Piston with piston shaft (6.2824.070 zircon piston or 6.2824.000 sapphire piston) 35 Inlet valve (6.2824.090) 36 Outlet valve (6.2824.080) 28 Spring retainer 37 Screw holder for valve. 29 Spring (6.2824.050) (for main piston) or Spring (6.2824.060) (for auxiliary piston) 38 Special tool (6.2617.010) to remove the piston seal 34.
4 Notes – Maintenance – Faults 5 Cleaning/Replacement of inlet valve 35 and outlet valve 36 Contaminated or blocked valves are cleaned by rinsing with dist. water, RBS solution or acetone. The rinsing effect can be reinforced by brief treatment in an ultrasonic bath (max. 20 s; if longer the sapphire sphere of the valve can be damaged). If this does not have the desired effect, the valves can be disassembled as shown in Fig. 10. Therefore the valves are inserted into the holder of 6.2617.
4.2 Maintenance and servicing Inlet valve 6.2824.090 Outlet valve 6.2824.080 40 40 40 Valve housing 41 Sealing ring (black) 42 Sleeve 43 Sapphire sleeve The bright side must point towards the sapphire sphere 41 41 42 42 44 Sapphire sphere 43 45 44 44 45 Ceramic holder for sapphire sphere The large recess must point in the direction of the sapphire sphere 45 43 46 46 Fig.
4 Notes – Maintenance – Faults 4.3 Faults and malfunctions If difficulties appear with the IC system during analyses, their causes are best investigated in the order separating column → 818 IC Pump → eluent → 819/820 IC System (see 819/820 Instructions for Use, section Faults and malfunctions). Several of the malfunctions which may appear with the 818 IC Pump are listed in the following table with details of possible causes and countermeasures.
5.1 RS 232 interface 5 Interfaces 5.1 RS 232 interface 5.1.1 Data transmission protocol The RS 232 interface of the 818 IC Pump is configured as DTE (Data Terminal Equipment) with the following technical specifications: • Standard Data interface in accordance with EIA standard RS 232C (DIN 66020, page 1) • Baud rate 9600 • Data Bits 8 • Stopp Bits 1 • XON/XOFF off • Control characters CR LF • Max.
5 Interfaces 5.1.2 Pin assignment RS 232C interface extern Transmitted Data (TxD) If no data transmission takes place, the line is maintained in the ”ON” condition. Data are sent only when CTS and DSR are in the ”ON” condition and DCD is in the ”OFF” condition. Pin 2 Transmitted Data Received Data (RxD) Data are received only when DCD is ”ON”. Pin 3 Request to Send (RTS) ON condition: 818 IC Pump is ready to send data.
5.2 Control interface 5.2 Control interface 5.2.1 Functions The 818 IC Pump has the following control inputs and outputs, which are accessible via the control interface: Inputs Reduce flow rate via contact Stop pump via contact Outputs Contact open, when pump has been stopped You will find detailed information on these functions in the following section. 5.2.
5 Interfaces 818 IC Pump external Function Inputs + 5V Stop pump with contact Contact closed: Pump is stopped 100k 4.7k 8 1n 7 Outputs 3 Pump stopped Contact open: Contact closed: Relay Pump stopped Pump running 4 34 818 IC Pump / 8.818.
5.2 Control interface 818 IC Pump external Function Display of suction phase of the 818 IC Punp 5 6 9 Connection not used Contact arrangement at connector (male) for socket "Control" (female) 5 1 9 6 No liability whatsoever will be accepted for damage arising from the improper connection of devices. 818 IC Pump / 8.818.
6 Appendix 6 Appendix 6.1 Technical specifications Provided that nothing to the contrary is mentioned, the published data are typical values for the 818 IC Pump at an ambient temperature of 25°C. Type Serial dual piston with two valves Pump capacity Flow range 0.05...5.00 mL/min Flow accuracy < 1.0 % Flow constancy < 0.5 % (after unit warmed up) Reproducibility of eluent flow < 0.1 % Pressure Pressure range 0...30.0 MPa (0...300 bar) Resolution for pressure indicator 0.
6.1 Technical specifications Pump head Pump head volumes Main piston: Priming piston: 40 µL 20 µL Pump displacement volumes Main piston: Priming piston: 28.5 µL 14.25 µL Length of stroke 3.6 mm 1.8 mm Main piston: Priming piston: Programming Remote control Flow rate Maximum and minimum pressure limit values Correction factor for pump head Start/Stop Storage of entries Type Flash-ROM Duration > 20 years Remote control Interfaces RS 232 (syntax Metrohm, see section 5.
6 Appendix Safety specifications Construction / Testing According to EN/IEC 61010-1 / UL 3101-1, protection class 1, degree of protection IP40 Safety directions This Instructions for Use include information and warnings which must be heeded by the user to assure safe operation of the instrument.
6.2 Scope of delivery 6.2 Scope of delivery Subject to changes ! All dimensions are given in mm. The IC Pump 2.818.0110 (metal-free) includes the following parts: Quant. Order No. Description 1 6.1831.010 PEEK capillary Length = 3 m 1 6.1834.000 0.25 Aspirating tubing made of PTFE, with connector for 6.2821.090 Aspirating filter 1.5 1 ⁄16" 2.5 Length = 1.2 m For the connection 818 IC Pump – eluent container 1 1 6.2122.0X0 6.2617.
6 Appendix Quant. Order No. Description 1 6.2816.020 Syringe made of PP, volume = 10 mL with Luer connector 102 1 6.2816.040 Tubule with PTFE tubing and Luer connection For 6.2816.020 syringe 120 1 6.2821.090 Aspirating filter Pore dimension 20 µm ∅9 For 6.1834.000 Aspirating tubing. 35 Set of 5 1 6.2821.120 Filter unit PEEK 2 µm To avoid contamination due to abrasive particles of piston seals Spare part: 6.2821.130 Filter 1 6.2824.
6.3 Optional accessories 6.3 Optional accessories Order No. Description 6.1834.010 Aspirating tubing made of PTFE, with connector for 6.2821.090 Aspirating filter 1.5 2.5 Length = 2.5 m For the connection 818 IC Pump – eluent vessel of 6.5324.000 Bottle rack 6.2620.150 Pulsation dampener MF Metal-free pulsation dampener for reduction of pulsation and preservation of separating columns. 6.2621.080 Capillary tubing cutter for 6.1831.010 PEEK capillaries and 6.1822.
6 Appendix Order No. Description 6.2824.030 Sapphire supporting ring 1.3 Spare part for 6.2824.100 pump head ∅3.2 ∅6.3 6.2824.050 Spring for main piston Spare part for 6.2824.100 pump head ∅11 30 6.2824.060 Spring for auxiliary piston Spare part for 6.2824.100 pump head ∅11 47 6.2824.080 Outlet valve ∅8 Spare part for 6.2824.100 pump head 16 6.2824.090 Inlet valve ∅8 Spare part for 6.2824.100 pump head 16 6.2617.020 Special tool For dismantling the valves 6.5324.
6.3 Optional accessories Order No. Description 6.2125.110 RS 232 connection cable Connection cable 818 IC Pump – PC) 6.2125.060 RS 232 connection cable Connection cable 818 IC Pump – PC. 818 IC Pump / 8.818.
6 Appendix 6.4 Validation / GLP GLP (Good Laboratory Practice) requires, among other things, that the precision and correctness of analytical instruments is checked at regular intervals by using SOPs (Standard Operating Procedures, SOP). An example of such a standard operating procedure is available from Metrohm under the title «Application Bulletin No. 277 – Validation of Metrohm Ion Chromatography Systems by using Standard Operating Procedures (SOP)».
6.5 Warranty and Conformity 6.5 6.5.1 Warranty and Conformity Warranty The warranty on our products is limited to defects that are traceable to material, construction or manufacturing error which occur within 12 months from the day of delivery. In this case, the defects will be rectified in our workshops free of charge. Transport costs are to be paid by the customer. For day and night operation, the warranty is limited to 6 months.
6 Appendix 6.5.2 Declaration of Conformity This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for security and to system validation issued by the manufacturing company. CH-9101 Tel. Fax Herisau, Switzerland +41 71 353 85 85 +41 71 353 89 01 www.metrohm.com Name of commodity 818 IC Pump System software Stored in ROMs Name of manufacturer Metrohm Ltd.
6.5 Warranty and Conformity 6.5.3 Quality Management Principles Metrohm Ltd., CH-9101 Herisau, Switzerland CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com Metrohm Ltd. holds the ISO 9001 Certificate, registration number 10872-02, issued by SQS (Swiss Association for Quality and Management Systems). Internal and external audits are carried out periodically to assure that the standards defined by Metrohm’s QM Manual are maintained.
6 Appendix 6.6 Index 8 818 IC Pump Advanced...................................22 Links ...........................................21 program .....................................20 program instructions..................21 830 IC Interface Connection.................................13 A Abrasive particles ..........................23 ............................................21 Adjustable spanner (6.2621.000) ..39 Ambient temperature .....................38 Appendix ...............................
6.6 Index Figure .................................... 3 Interfaces ....................................... 31 Introduction ..................................... 1 IQ ................................................... 44 ISO 9100........................................ 46 Outlet valve 36 Cleaning..................................... 28 Components .............................. 29 Figure................................... 27, 29 Ordering designations............... 42 Replacement ...........................
6 Appendix Ordering designation.................42 Special tool 38 Figure .........................................27 Ordering designation.................39 Remove piston seal 34..............25 Special tool 39 Figure .........................................27 Install piston seal 34..................27 Ordering designation.................39 Spilled chemicals...........................24 Spring 29 6.2824.050 Figure...................................27 6.2824.060 Figure...................................